Polytetrafluoroethylene aqueous dispersion and its product
a technology of polytetrafluoroethylene and aqueous dispersion, applied in the field of polytetrafluoroethylene, can solve the problems of poor wettability and low permeability of obtained aqueous ptfe emulsion, insufficient physical properties of obtained ptfe, and tendency to be repelled, and achieve excellent wettability and mechanical stability
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reference example 1
Production Example of CF3CF2OCF(CF3)CF2OCF(CF3)COONH4
[0096]2.58 g of CsF and 13.06 g of tetraglyme were charged into a hastelloy c autoclave having a capacity of 200 mL, followed by degassing, and then, 20.83 g of CF3COF was introduced. Then, the autoclave was cooled to −20° C., and under a hermetically sealed and stirred condition, 57.5 g of hexafluoropropene oxide was introduced over a period of about one hour. The initial pressure showed 0.6 MPa. The reaction was continued for about one hour until the pressure no longer decreased, and then, the autoclave was returned to room temperature to obtain 78.57 g of a reaction crude liquid. This liquid was subjected to a GC analysis, whereby it was found that in addition to the objective product, 49.7% of CF3CF2OCF(CF3)CF2OCF(CF3)COF, 19.1% of CF3CF2OCF(CF3)COF and 12.8% of CF3CF2O(CF(CF3)CF2O)2CF(CF3)COF, were contained.
[0097]The same reaction was carried out by using 32.26 g of CF3COF. Distillation and purification were carried out by ...
reference example 2
Measurement of 1-Octanol / Water Partition Coefficient (LogPOW)
[0099]In accordance with OECD Test Guideline 117, 1-octanol / water partition coefficient (LogPOW) of a fluorinated emulsifier was measured by using HPLC (high performance liquid chromatography).
[0100]Conditions for the measurement were as follows: column: TOSOH ODS-120T column (φ 4.6 mm×250 mm), eluent: acetonitrile / 0.6 mass % of HClO4 solution=1 / 1 (vol / vol %), flow rate: 1.0 m / minute, sample amount: 300 μL, column temperature: 40° C., and detection light: UV 210 nm (WO2005-42593).
[0101]HPLC was carried out on standard substances (heptanoic acid, octanoic acid, nonanoic acid and decanoic acid) having known 1-octanol / water partition coefficients, and a calibration curve was prepared from the respective elution times and octanol / water partition coefficients of the respective standard substances. Based on this calibration curve, a value of partition coefficient (LogPOW) between 1-octanol and water was calculated from the eluti...
example 1
[0105]EEA was used as the fluorinated emulsifier. Into a 100 L stainless steel autoclave equipped with a baffle plate and a stirrer, 36 g of EEA, 555 g of paraffin wax (melting point: 55° C.) and 61.3 liters of deionized water were charged. The air in the autoclave was replaced with nitrogen, and then the pressure was reduced. Then, a TFE monomer was added and the temperature was increased to 62° C. with stirring. In addition, the TFE monomer was injected until the inner pressure was raised to 1.765 MPa, and 26.3 g of disuccinic acid peroxide (concentration: 80 mass %, the rest being water) was dissolved in 1 L of warm water at about 70° C. and was injected into the autoclave.
[0106]About 3 minutes later, the inner pressure of the autoclave decreased to 1.716 MPa, whereupon the TFE monomer was injected to keep the inner pressure at 1.765 MPa and to let the polymerization proceed. EEA was dissolved in warm water, and the total of 53 g as EEA was added dividedly in two steps during the...
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